The synthetic method of 2-pyridinemethanol
A pyridinemethanol and synthesis method technology, applied in the direction of organic chemistry and the like, can solve the problems of complicated post-processing, many reaction by-products, long reaction time, etc., and achieve the effects of shortening reaction time, high yield and purity, and improving activation performance
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Embodiment 1
[0026] The synthetic method of 2-pyridinemethanol is characterized in that, comprises the following steps of synthesis:
[0027] 1) Synthesis of 2-methyl-3,5-dinitropyridine
[0028] Take 23.25g of 2-picoline as the synthetic raw material, add 24.8ml of 98% concentrated sulfuric acid to it, stir and raise the temperature to 70°C, then add 75.6ml of mixed acid dropwise therein, after the dropwise addition, raise the temperature to 90-92°C and keep it warm for 2.2h, then Cool in an ice-water bath, add 250mL of ice water to it, add dropwise 23.2g of 30% sodium hydroxide solution for neutralization, stir for 1.5h, then extract with ethyl acetate, recover the solvent by distillation under reduced pressure, and use organic reagents for recrystallization , filtered and dried to obtain 43.21 g of 2-methyl-3,5-dinitropyridine with a yield of 94.4%;
[0029] 2) Synthesis of 2-methyl-3,5-dinitropyridine-N-oxide
[0030] Take 36.62g of 2-methyl-3,5-dinitropyridine prepared in step 1) an...
Embodiment 2
[0036] The synthetic method of 2-pyridinemethanol is characterized in that, comprises the following steps of synthesis:
[0037] 1) Synthesis of 2-methyl-3,5-dinitropyridine
[0038] Take 18.6g of 2-picoline as the raw material for synthesis, add 19.2ml of 98% concentrated sulfuric acid to it, stir and raise the temperature to 70°C, then add 58.7ml of mixed acid dropwise therein, after the dropwise addition, raise the temperature to 90-92°C and keep it warm for 2.5h, then Cool in an ice-water bath, add 250 mL of ice water therein, add 18.2 g of 30% sodium hydroxide solution dropwise for neutralization, stir for 1 h, then extract with ethyl acetate, recover the solvent by distillation under reduced pressure, and use organic reagents for recrystallization, Suction filtration and drying yielded 35.19 g of 2-methyl-3,5-dinitropyridine with a yield of 96.1%;
[0039] 2) Synthesis of 2-methyl-3,5-dinitropyridine-N-oxide
[0040] Take 29.3g of 2-methyl-3,5-dinitropyridine prepared ...
Embodiment 3
[0046] The synthetic method of 2-pyridinemethanol is characterized in that, comprises the following steps of synthesis:
[0047] 1) Synthesis of 2-methyl-3,5-dinitropyridine
[0048] Take 32.74g of 2-picoline as a synthetic raw material, add 31.5ml of 98% concentrated sulfuric acid to it, stir and raise the temperature to 70°C, then add 100ml of mixed acid dropwise, after the addition is completed, heat up to 90-92°C and keep it warm for 1.8h, then ice Cool in a water bath, add 250mL of ice water to it, add dropwise 32.6g of 30% sodium hydroxide solution for neutralization, stir for 1 h, then extract with ethyl acetate, recover the solvent by distillation under reduced pressure, and use organic reagents for recrystallization, pumping Filter and dry to obtain 52.35 g of 2-methyl-3,5-dinitropyridine with a yield of 95.3%;
[0049] 2) Synthesis of 2-methyl-3,5-dinitropyridine-N-oxide
[0050] Take 45.78g of 2-methyl-3,5-dinitropyridine prepared in step 1) and add it to 100ml of...
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